CN108865373A - A kind of complex calcium sulfonate polyureas mixed grease and preparation method thereof - Google Patents

A kind of complex calcium sulfonate polyureas mixed grease and preparation method thereof Download PDF

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Publication number
CN108865373A
CN108865373A CN201810882354.1A CN201810882354A CN108865373A CN 108865373 A CN108865373 A CN 108865373A CN 201810882354 A CN201810882354 A CN 201810882354A CN 108865373 A CN108865373 A CN 108865373A
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calcium sulfonate
complex calcium
polyureas
grease
mixed grease
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CN201810882354.1A
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CN108865373B (en
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周宏光
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Hangzhou Xingang Lubrication Technology Co Ltd
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Hangzhou Xingang Lubrication Technology Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M169/00Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
    • C10M169/04Mixtures of base-materials and additives
    • C10M169/044Mixtures of base-materials and additives the additives being a mixture of non-macromolecular and macromolecular compounds
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M169/00Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
    • C10M169/06Mixtures of thickeners and additives
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2203/00Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions
    • C10M2203/04Well-defined cycloaliphatic compounds
    • C10M2203/045Well-defined cycloaliphatic compounds used as base material
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2205/00Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
    • C10M2205/02Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers
    • C10M2205/026Butene
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2217/00Organic macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2217/04Macromolecular compounds from nitrogen-containing monomers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2217/045Polyureas; Polyurethanes
    • C10M2217/0456Polyureas; Polyurethanes used as thickening agents
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2219/00Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
    • C10M2219/04Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions containing sulfur-to-oxygen bonds, i.e. sulfones, sulfoxides
    • C10M2219/044Sulfonic acids, Derivatives thereof, e.g. neutral salts
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/06Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2050/00Form in which the lubricant is applied to the material being lubricated
    • C10N2050/10Semi-solids; greasy

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Lubricants (AREA)

Abstract

The invention discloses a kind of complex calcium sulfonate polyureas mixed greases and preparation method thereof, and the weight proportion of raw material is as follows:Account for the mineral base oil of lubricating grease weight 50~70%, the carbamido thickening agent of lubricating grease weight 5~10% and the complex calcium sulfonate for accounting for lubricating grease weight 20~40%, also the polyisobutene tackifier comprising accounting for lubricating grease weight 5~15%.Product of the present invention maintains the fundamental characteristics such as urea-base grease dropping point is high, easily pump, antioxygen is anticorrosive; the advantage that complex calcium sulfonate base lubricating agent water-resistance is good, extreme-pressure wear-resistant is strong is merged; overcome complex calcium sulfonate grease ash content mostly easily coking plugging the drawbacks of; crucial emphasis is that solve common urea-base grease shearing property shortcoming, directly contact easily emulsification losing issue with water; the protection to mechanical equipment can be effectively improved, the service life of equipment is conducive to extend.

Description

A kind of complex calcium sulfonate polyureas mixed grease and preparation method thereof
Technical field
The invention discloses a kind of complex calcium sulfonate polyureas mixed greases and preparation method thereof, belong to lubricating grease synthesis skill Art field.
Background technique
With the raising increasingly that society requires quality of the life, just safer, environmentally friendly, comfortable to means of livelihood proposition, The individual requirements such as beauty.The processing of the means of livelihood be unable to do without high-accuracy mechanical equipment, the long-time good operation of mechanical equipment Lubricant grease is needed to protect.Common urea-base grease is used widely for a long time as high-quality lubriation material.But common urea Base grease shearing shortcoming directly contact with water and easily to emulsify losing issue to actually use process drawback more obvious.The present invention Complex calcium sulfonate polyureas mixed grease be exactly to solve specific question existing for common urea-base grease.Domestic some scientific research machines Structure and enterprise technique center are also in succession to urea-base grease, complex calcium sulfonate grease, complex calcium sulfonate-calcium naphthenate polyureas Lubricating grease has carried out a series of more in-depth studies, as 1087025 C of Research Institute of Petro-Chemical Engineering CN disclose it is a kind of high The preparation method of dropping point diurea grease lubricant;A kind of sulfoacid calcium-calcium naphthenate polyureas lubrication has been declared by Research Institute of Petro-Chemical Engineering The patent of rouge and preparation method;A kind of four polyurea grease of high base number calcium mahogany sulfonate base has been declared by Research Institute of Petro-Chemical Engineering And the patent of preparation method;Research Institute of Petro-Chemical Engineering 20121004197 has applied for a kind of six polyurea grease of composite calcium-base And preparation method thereof.Although being all polyurea grease patent of invention and preparation method thereof, above-mentioned patent, which has no, to be addressed in urea groups Rouge reaction process directly adds the factory formula and preparation method of complex calcium sulfonate grease ingredient.
Summary of the invention
An object of the present invention is to overcome above-mentioned the shortcomings of the prior art and provide a kind of complex calcium sulfonate polyureas Mixed grease.
The second object of the present invention is to provide a kind of preparation method of complex calcium sulfonate polyureas mixed grease, this method can It solves the problems, such as to commonly use areidofat shearing shortcoming, directly contact easily emulsification loss with water.
The present invention solves technical problem, and the technical solutions adopted are as follows:
A kind of complex calcium sulfonate polyureas mixed grease, the weight proportion of raw material are as follows:Account for lubricating grease weight 50~ 70% mineral base oil, the carbamido thickening agent of lubricating grease weight 5~10% and the compound sulphur for accounting for lubricating grease weight 20~40% Sour calcium, also the polyisobutene tackifier comprising accounting for lubricating grease weight 5~15%.
Advanced optimize proportion can be as:Mineral base oil, carbamido thickening agent, complex calcium sulfonate, polyisobutene are by weight Measuring percentage is 61%, 6%, 25%, 8% respectively.
Mineral oil base oil is made of BS series.Carbamido thickening agent is reacted by amine and isocyanates.Complex calcium sulfonate Base grease is screened by No. 0, No. 1, No. 2, No. 3 consistency.Polyisobutene has molecular weight 9500 (abbreviation PB950), 13000 (abbreviation PB1300), 24000 (abbreviation PB2400) series are screened.Water (accounting for the 3% of lubricating grease weight, be not counted in formula) is only Make cosolvent use, all volatilization removings after high-temperature heating.
Mineral base oil as component is the one kind of high-pressure hydrogenation series bright stock (i.e. 150BS, 175BS, 250BS etc.) Or two kinds of mixtures.Its technical indicator of BS series base oil is:40 DEG C of 400~800mm2/s of kinematic viscosity, viscosity index (VI) be not low In 90, flash-point is not less than 250 DEG C.BS base oil account for total complex calcium sulfonate polyureas mixed grease weight percent be 50~ 70%.
Carbamido thickening agent as component is one kind of organic amine (octadecylamine, cyclohexylamine, aniline, para-totuidine etc.), two It plants or three kinds is reacted to be formed with toluene di-isocyanate(TDI).Organic amine is preferably the mixture of octadecylamine and cyclohexylamine.Octadecylamine, The mutual optimization molar ratio of cyclohexylamine, toluene di-isocyanate(TDI) is (0.5~1.5): (0.5~2): (0.5~2), further excellent Change than that can be such as 1: 1: 1.The weight percent that carbamido thickening agent accounts for is 5~10%.
Complex calcium sulfonate grease as component is No. 0, No. 1, No. 2, No. 3 consistency screen.Instant component Preferably No. 2, No. 3 consistency complex calcium sulfonate greases of total weight 20~35%, advanced optimize than account for total weight 22 ~30%.
As component tackifier polyisobutene be molecular weight 9500 (abbreviation PB950), 13000 (abbreviation PB1300), 24000 (abbreviation PB2400) series are screened.Instant component is preferably PB1300, the PB2400 for accounting for total weight 5~15%, Advanced optimize than account for total weight 5~10%.
The technology of preparing of tasteless urea-base grease of the present invention, key step are as follows:
1) mineral base oil, complex calcium sulfonate grease being added in reaction kettle first, stirring is warming up to 65-75 DEG C, Isocyanate compound, then insulated and stirred 30-60min is added, is slowly added into the case where keeping stirring heat preservation organic aminated Object is closed, 60-90min is stirred to react;
2) continue to heat up, in 90-100 DEG C of insulation reaction 60-90min;
3) water stirring constant temperature is added in 100-110 DEG C of range, keeps 30-60min;
4) continue to be warming up to 170-185 DEG C, constant temperature stirring keeps 10-30min;
5) for rapid cooling to 100 DEG C hereinafter, polyisobutene tackifier are added, constant temperature stirs 60-90min;
6) finally it is ground into rouge.
Complex calcium sulfonate polyureas mixed lubrication fat prod of the invention has the advantages that:Technology of preparing of the present invention can solve Common areidofat shearing shortcoming directly contacts the problem of easily emulsification is lost with water.
Specific embodiment
Below with reference to embodiment, the present invention is described in further detail.The specific embodiment of the invention is essentially identical, Only specific ratio quantity and specific raw material are different.
Embodiment 1
A kind of complex calcium sulfonate polyureas mixed grease, by 305 grams of 150BS, 125 grams of No. 2 complex calcium sulfonate greases It being added in reaction vessel, stirring is warming up to 68-73 DEG C, 12.2 grams of toluene di-isocyanate(TDI)s, then insulated and stirred 30min are added, 13.0 grams of octadecylamines, 4.8 grams of cyclohexylamine are slowly added into the case where keeping stirring, insulated and stirred reacts 75min, continues to be warming up to 15 grams of water are added in 93-98 DEG C of insulation reaction 75min, in 103-108 DEG C of insulation reaction 45min, continue to be warming up to 180 DEG C, constant temperature Stirring keeps 20min, and to 100 DEG C hereinafter, 40 grams of polyisobutene PB2400 are added, constant temperature stirring 60min. is finally ground rapid cooling It wears into rouge analysis data and is shown in Table 1.
Embodiment 2
A kind of complex calcium sulfonate polyureas mixed grease, by 290 grams of 150BS, 140 grams of No. 2 complex calcium sulfonate greases It being added in reaction vessel, stirring is warming up to 68-73 DEG C, 16.2 grams of toluene di-isocyanate(TDI)s, then insulated and stirred 30min are added, 17.4 grams of octadecylamines, 6.4 grams of cyclohexylamine are slowly added into the case where keeping stirring, insulated and stirred reacts 75min, continues to be warming up to 15 grams of water are added in 93-98 DEG C of insulation reaction 75min, in 103-108 DEG C of insulation reaction 45min, continue to be warming up to 180 DEG C, constant temperature Stirring keeps 20min, and to 100 DEG C hereinafter, 30 grams of polyisobutene PB2400 are added, constant temperature stirring 60min. is finally ground rapid cooling It wears into rouge analysis data and is shown in Table 1.
Embodiment 3
A kind of complex calcium sulfonate polyureas mixed grease, by 315 grams of 150BS, 110 grams of No. 3 complex calcium sulfonate greases It being added in reaction vessel, stirring is warming up to 68-73 DEG C, 14.2 grams of toluene di-isocyanate(TDI)s, then insulated and stirred 30min are added, 15.2 grams of octadecylamines, 5.6 grams of cyclohexylamine are slowly added into the case where keeping stirring, insulated and stirred reacts 75min, continues to be warming up to 15 grams of water are added in 93-98 DEG C of insulation reaction 75min, in 103-108 DEG C of insulation reaction 45min, continue to be warming up to 180 DEG C, constant temperature Stirring keeps 20min, and to 100 DEG C hereinafter, 40 grams of polyisobutene PB1300 are added, constant temperature stirring 60min. is finally ground rapid cooling It wears into rouge analysis data and is shown in Table 1.
Embodiment 4
A kind of complex calcium sulfonate polyureas mixed grease, by 295 grams of 150BS, 125 grams of No. 3 complex calcium sulfonate greases It being added in reaction vessel, stirring is warming up to 68-73 DEG C, 20.5 grams of toluene di-isocyanate(TDI)s, then insulated and stirred 30min are added, 22 grams of octadecylamines, 7.5 grams of aniline are slowly added into the case where keeping stirring, insulated and stirred reacts 75min, continues to be warming up to 93- 15 grams of water are added in 98 DEG C of insulation reaction 75min, in 103-108 DEG C of insulation reaction 45min, continue to be warming up to 180 DEG C, constant temperature stirs It mixes and keeps 20min, to 100 DEG C hereinafter, 40 grams of polyisobutene PB2400 are added, constant temperature stirring 60min. is finally ground rapid cooling 1 is shown in Table at rouge analysis data.
In addition to the implementation, the present invention can also have other embodiments.It is all to use equivalent substitution or equivalent transformation shape At technical solution, fall within the scope of protection required by the present invention.

Claims (10)

1. a kind of complex calcium sulfonate polyureas mixed grease, which is characterized in that the weight percent composition of its raw material is as follows:50~ 70% mineral base oil, 5~10% carbamido thickening agent, 20~40% complex calcium sulfonate grease and 5~15% Polyisobutene tackifier.
2. complex calcium sulfonate polyureas mixed grease according to claim 1, which is characterized in that the weight percent of its raw material It forms as follows:61% mineral base oil, 6% carbamido thickening agent, 25% complex calcium sulfonate grease and 8% polyisobutene thickening Agent.
3. complex calcium sulfonate polyureas mixed grease according to claim 1 or claim 2, which is characterized in that the mineral base oil Any one in high-pressure hydrogenation BS bright stock or two kinds of mixtures.
4. complex calcium sulfonate polyureas mixed grease according to claim 3, which is characterized in that the mineral base oil is selected from Any one in 150BS, 175BS and 250BS bright stock or two kinds of mixtures.
5. complex calcium sulfonate polyureas mixed grease according to claim 1 or claim 2, which is characterized in that the carbamido thickening agent It reacts to be formed for organic amine and toluene di-isocyanate(TDI), the organic amine is in octadecylamine, cyclohexylamine, aniline and para-totuidine Any one, two kinds or three kinds.
6. complex calcium sulfonate polyureas mixed grease according to claim 1 or claim 2, which is characterized in that organic amine is octadecylamine Molar ratio with the mixture of cyclohexylamine, octadecylamine, cyclohexylamine and toluene di-isocyanate(TDI) is (0.5~1.5): (0.5~2): (0.5~2).
7. complex calcium sulfonate polyureas mixed grease according to claim 6, which is characterized in that octadecylamine, cyclohexylamine and first The molar ratio of phenylene diisocyanate is 1: 1: 1.
8. complex calcium sulfonate polyureas mixed grease according to claim 1, which is characterized in that the polyisobutene tackifier It is made of molecular weight 9500,13000 and 24000 series.
9. complex calcium sulfonate polyureas mixed grease according to claim 8, which is characterized in that the polyisobutene tackifier It is made of the series of molecular weight 9500 and 24000.
10. the preparation method of complex calcium sulfonate polyureas mixed grease described in a kind of claim 1, which is characterized in that step is such as Under:
1) mineral base oil, complex calcium sulfonate grease are added in reaction kettle first, stirring is warming up to 65-75 DEG C, is added Isocyanate compound, then insulated and stirred 30-60min are slowly added into organic amine compound in the case where keeping stirring heat preservation, It is stirred to react 60-90min;
2) continue to heat up, in 90-100 DEG C of insulation reaction 60-90min;
3) water stirring constant temperature is added in 100-110 DEG C of range, keeps 30-60min;
4) continue to be warming up to 170-185 DEG C, constant temperature stirring keeps 10-30min;
5) for rapid cooling to 100 DEG C hereinafter, polyisobutene tackifier are added, constant temperature stirs 60-90min;
6) finally it is ground into rouge.
CN201810882354.1A 2018-08-05 2018-08-05 Composite calcium sulfonate polyurea mixed lubricating grease and preparation method thereof Active CN108865373B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110511806A (en) * 2019-07-10 2019-11-29 杭州新港润滑科技有限公司 A kind of high temperature water resistant urea-base grease and its preparation process
CN114672363A (en) * 2021-12-25 2022-06-28 科特龙流体科技(扬州)有限公司 Pumpability lubricating grease and preparation method thereof

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Publication number Priority date Publication date Assignee Title
CN110511806A (en) * 2019-07-10 2019-11-29 杭州新港润滑科技有限公司 A kind of high temperature water resistant urea-base grease and its preparation process
CN110511806B (en) * 2019-07-10 2021-10-01 杭州新港润滑科技有限公司 High-temperature water-resistant carbamido lubricating grease and preparation process thereof
CN114672363A (en) * 2021-12-25 2022-06-28 科特龙流体科技(扬州)有限公司 Pumpability lubricating grease and preparation method thereof

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